CN111760561A - Preparation method of As (III) ion imprinted material based on MCM-41 molecular sieve surface - Google Patents
Preparation method of As (III) ion imprinted material based on MCM-41 molecular sieve surface Download PDFInfo
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Abstract
The invention discloses a preparation method of an As (III) ion imprinted material based on the surface of an MCM-41 molecular sieve. The method takes N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane As a functional monomer, epichlorohydrin As a cross-linking agent and an MCM-41 molecular sieve As a carrier, and adopts a surface imprinting method to prepare the As (III) ion imprinting material based on the surface of the MCM-41 molecular sieve. The As (III) ion imprinted material based on the MCM-41 molecular sieve surface has a specific three-dimensional cavity structure, is good in mechanical property and easy to elute, can be used for specific recognition and selective removal of As (III) ions in an aqueous solution, and has the advantages of low cost, environmental protection and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of environment functional materials, and particularly relates to a preparation method of an As (III) ion imprinted material based on the surface of an MCM-41 molecular sieve.
Background
As (III) ions have high toxicity and easily generate enrichment effect on aquatic organisms and human bodies, thereby causing teratogenesis, carcinogenesis and mutagenic three-cause harm. Most of the traditional treatment methods adopt an adsorption method, have the advantages of low cost and simple operation, but lack pertinence and great blindness to target ions, so that research and development of an adsorption material with selective separation to the target ions are particularly important.
The ion imprinting technology is a technology with selective and specific recognition function on target ions, and the ion imprinting polymer is a rigid polymer with cavities with specific shapes and sizes, which is formed by taking anions and cations as templates, reacting with functional monomers through special coordination, complexation or electrostatic interaction and the like, further performing cross-linking polymerization, and removing the template ions by adopting a physical or chemical method. According to the traditional ion imprinting preparation method, recognition sites are distributed in an imprinting material, and a part of the recognition sites are embedded too deeply, so that template ions cannot reach to form failure sites, and the defects of low mass transfer speed and difficult elution exist. The surface ion imprinting technology is a novel ion imprinting technology which is rapidly developed on the basis of the traditional ion imprinting preparation technology, and almost all recognition sites are designed on the surface of a carrier by adopting certain measures, so that the mass transfer effect between the recognition sites and target ions is improved, the elution and recombination of the target ions are facilitated, and the defects of the traditional method are effectively avoided.
The surface ion imprinting technology is used for preparing the imprinting material, and the carrier can increase the surface area, the mechanical strength, the thermal stability and other characteristics of the imprinting polymer to improve the adsorption performance of the imprinting material. The selection of the carrier is particularly important, the MCM-41 mesoporous molecular sieve has the characteristics of large specific surface area, large macroporous volume, large adsorption capacity, high porosity, narrow pore size distribution, rich hydroxyl on the surface, ordered long-range structure, easy control of pore size and the like, can be used for chemical modification, is an ideal imprinted carrier, and the surface imprinted adsorption material synthesized by using the MCM-41 molecular sieve as an imprinted substrate has the advantages of high selectivity and high identification on template ions, low cost and environmental protection.
Disclosure of Invention
The invention aims to provide a preparation method of an As (III) ion imprinted material based on the surface of an MCM-41 molecular sieve. The method has the advantages of low cost, environmental protection, high selectivity and high identification on target ions, and the target ions are As (III) ions.
The method comprises the following specific steps:
(1) preparation of MCM-41: 1.2g of cetyltrimethylammonium bromide was weighed into a three-necked flask, and at the same time, 90mL of ammonia water and 130mL of distilled water were weighed and added to the three-necked flask. Stirring at 60 ℃ until the cetyltrimethylammonium bromide is completely dissolved. Under the condition of vigorous stirring, slowly dropwise adding 5mL of tetraethoxysilane, then stirring at a constant speed, and reacting for 6 h. Stopping the reaction, pouring out while the reaction is hot, and crystallizing for 3d at room temperature. The solid particles are washed to neutrality and dried. Burning the mixture for 6 hours at 550 ℃ in a muffle furnace to remove hexadecyl trimethyl ammonium bromide to obtain MCM-41;
(2) weighing 0.2-0.3mmol of sodium arsenite solid in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the sodium arsenite solid, weighing 80-100mL of absolute ethanol, adding the absolute ethanol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, then adding 1g of MCM-41 obtained in the step (1), condensing and refluxing at 60-80 ℃ for 20h, then adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, performing suction filtration, and washing for 2-3 times by using the absolute ethanol;
(3) and (3) finally, adding 2mol/L hydrochloric acid in the step (2) to elute for 2-4h at normal temperature, washing with deionized water to be neutral, and drying at 80 ℃ to obtain the As (III) ion imprinted material based on the surface of the MCM-41 molecular sieve.
The method has the beneficial effects that the method adopts a surface imprinting method, takes the MCM-41 molecular sieve with large specific surface area, good mechanical property and stability and containing a large amount of silicon hydroxyl on the surface As a carrier, takes N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane As a functional monomer, takes epoxy chloropropane As a cross-linking agent, prepares the As (III) ion imprinting material based on the surface of the MCM-41 molecular sieve through polymerization, and is applied to the research on As (III) ionsThe adsorption capacity of 0mg/LAs (III) ion reaches 96.89%, has better adsorption and Cl resistance-、NO3 -、SO4 2-、HPO4 2-The selectivity coefficient of the catalyst can reach more than 1.5, and the catalyst has good selectivity.
Detailed Description
The present invention is further illustrated by the following examples and comparative examples, but the following descriptions are only illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1:
an As (III) ion imprinting material based on MCM-41 molecular sieve surface comprises the following steps:
(1) preparation of MCM-41: 1.2g of cetyltrimethylammonium bromide was weighed into a three-necked flask, and at the same time, 90mL of ammonia water and 130mL of distilled water were weighed and added to the three-necked flask. Stirring at 60 ℃ until the cetyltrimethylammonium bromide is completely dissolved. Under the condition of vigorous stirring, slowly dropwise adding 5mL of tetraethoxysilane, then stirring at a constant speed, and reacting for 6 h. Stopping the reaction, pouring out while the reaction is hot, and crystallizing for 3d at room temperature. The solid particles are washed to neutrality and dried. Burning the mixture for 6 hours at 550 ℃ in a muffle furnace to remove hexadecyl trimethyl ammonium bromide to obtain MCM-41;
(2) weighing 0.2mmol of sodium arsenite solid in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the sodium arsenite solid, weighing 80-100mL of absolute ethyl alcohol, adding the absolute ethyl alcohol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, adding 1g of MCM-41 obtained in the step (1), condensing and refluxing at 60 ℃ for 20h, adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, carrying out suction filtration, and washing for 2-3 times by using the absolute ethyl alcohol;
(3) and (3) finally, adding 2mol/L hydrochloric acid in the step (2) to elute for 2-4h at normal temperature, washing with deionized water to be neutral, and drying at 80 ℃ to obtain the As (III) ion imprinted material (MCM-41-IIP1) based on the surface of the MCM-41 molecular sieve.
Comparative example 1:
the remaining preparation steps were the same as in example 1 except that no sodium arsenite was added in step (2) to obtain a non-imprinted adsorbent material (MCM-41-NIP 1).
Example 2:
(1) preparation of MCM-41: 1.2g of cetyltrimethylammonium bromide was weighed into a three-necked flask, and at the same time, 90mL of ammonia water and 130mL of distilled water were weighed and added to the three-necked flask. Stirring at 60 ℃ until the cetyltrimethylammonium bromide is completely dissolved. Under the condition of vigorous stirring, slowly dropwise adding 5mL of tetraethoxysilane, then stirring at a constant speed, and reacting for 6 h. Stopping the reaction, pouring out while the reaction is hot, and crystallizing for 3d at room temperature. The solid particles are washed to neutrality and dried. Burning the mixture for 6 hours at 550 ℃ in a muffle furnace to remove hexadecyl trimethyl ammonium bromide to obtain MCM-41;
(2) weighing 0.25mmol of sodium arsenite in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the sodium arsenite, weighing 80-100mL of methanol, adding the methanol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, then adding g of MCM-41 obtained in the step (1), condensing and refluxing at 70 ℃ for 20h, then adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, carrying out suction filtration, and washing for 2-3 times by using absolute ethyl alcohol;
(3) and (3) finally, adding 2mol/L hydrochloric acid in the step (2) to elute for 2-4h at normal temperature, washing with deionized water to be neutral, and drying at 80 ℃ to obtain the As (III) ion imprinted material based on the surface of the MCM-41 molecular sieve. (MCM-41-IIP 2);
the rest preparation steps are the same as the example 2, except that the sodium arsenite is not added in the step (2), and the mesoporous MCM-41 non-imprinted adsorption material (MCM-41-NIP2) is prepared.
Example 3:
(1) preparation of MCM-41: 1.2g of cetyltrimethylammonium bromide was weighed into a three-necked flask, and at the same time, 90mL of ammonia water and 130mL of distilled water were weighed and added to the three-necked flask. Stirring at 60 ℃ until the cetyltrimethylammonium bromide is completely dissolved. Under the condition of vigorous stirring, slowly dropwise adding 5mL of tetraethoxysilane, then stirring at a constant speed, and reacting for 6 h. Stopping the reaction, pouring out while the reaction is hot, and crystallizing for 3d at room temperature. The solid particles are washed to neutrality and dried. Burning the mixture for 6 hours at 550 ℃ in a muffle furnace to remove hexadecyl trimethyl ammonium bromide to obtain MCM-41;
(2) weighing 0.3mmol of sodium arsenite solid in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the sodium arsenite solid, weighing 80-100mL of methanol, adding the methanol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, then adding 1g of MCM-41 obtained in the step (1), condensing and refluxing at 80 ℃ for 20h, then adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, carrying out suction filtration, and washing for 2-3 times by using absolute ethyl alcohol;
(3) finally, 2mol/L hydrochloric acid is added in the step (2) to elute for 2-4h at normal temperature, then deionized water is used for washing until the solution is neutral, and drying is carried out at 80 ℃ to obtain an As (III) ion imprinting material (MCM-41-IIP3) based on the surface of the MCM-41 molecular sieve;
the rest preparation steps are the same as those of the example 3, except that the sodium arsenite is not added in the step (2), and the mesoporous MCM-41 non-imprinted adsorption material (MCM-41-NIP3) is prepared.
Adsorption experiment:
0.01g of adsorbent was weighed and added to 20mL of 50mg/L ionic solution (As (III), Cl, respectively)-、NO3 -、SO4 2-、HPO4 2-) The resulting mixture was adsorbed at 25 ℃ for 2 hours, filtered through a 0.45-. mu.m filter membrane, and the ion concentration of the filtrate was measured. According to the change of the ion concentration before and after adsorption, the ion removal rate was calculated as follows:
in the formula: c0: pre-adsorption ion concentration (mg/L); ce: ion concentration (mg/L) after adsorption equilibration.
The samples obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to the above adsorption test, respectively, and the results are shown in the table:
from the above table, the maximum removal rate of As (III) ions by the As (III) ion imprinted material based on the MCM-41 molecular sieve surface prepared by the embodiment of the invention is 96.89%, and the maximum removal rate is obviously higher than the removal rate of As (III) ions by the non-imprinted adsorption material and the removal rate of other ions by the imprinted adsorption material, and the method can be used for specific recognition and selective removal of As (III) ions.
Claims (1)
1. A method for preparing an As (III) ion imprinted material based on the surface of an MCM-41 molecular sieve is characterized by comprising the following specific steps:
(1) preparation of MCM-41: weighing 1.2g of hexadecyl trimethyl ammonium bromide into a three-neck flask, simultaneously weighing 90mL of ammonia water and 130mL of distilled water, adding the ammonia water and the distilled water into the three-neck flask together, stirring at 60 ℃ until the hexadecyl trimethyl ammonium bromide is completely dissolved, slowly dropwise adding 5mL of ethyl orthosilicate under vigorous stirring, stirring at a constant speed, reacting for 6 hours, stopping the reaction, pouring out while the reaction is hot, crystallizing for 3 days at room temperature, washing the solid particles to be neutral, drying, and burning for 6 hours at 550 ℃ in a muffle furnace to remove the hexadecyl trimethyl ammonium bromide, thereby obtaining MCM-41;
(2) weighing 0.2-0.3mmol of sodium arsenite solid in a three-necked bottle, adding 10mL of ultrapure water to fully dissolve the sodium arsenite solid, weighing 80-100mL of absolute ethanol, adding the absolute ethanol into the three-necked bottle, uniformly mixing, dropwise adding 2mL of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, reacting for 1-2h, then adding 1g of MCM-41 obtained in the step (1), condensing and refluxing at 60-80 ℃ for 20h, then adding 1.44mL of epoxy chloropropane, continuing to react for 2-4h, cooling, performing suction filtration, and washing for 2-3 times by using the absolute ethanol;
(3) and (3) finally, adding 2mol/L hydrochloric acid in the step (2) to elute for 2-4h at normal temperature, washing with deionized water to be neutral, and drying at 80 ℃ to obtain the As (III) ion imprinted material based on the surface of the MCM-41 molecular sieve.
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